Psychologická laboratoř CASRI

The CASRI Psychological Laboratory is part of the scientific and service department of the Physical Education and Sport, which provides service, methodological, advisory, and consultancy services. The laboratory is involved in research tasks aimed at the development and validation of methods selection and training of military personnel for the needs of the Ministry of Defence and the Czech Army of the Czech Republic. It is also involved in educational and methodological activities. In addition to research activities provides support to top athletes from the national sports team and their coaches.

Validation of Methods for Estimation of Knee Joint Mechanical Impedance During Locomotion Using a Torque-Controllable Knee Exoskeleton

The mechanical impedance of the joints of the leg govern the body's response to external disturbances, and its regulation is essential for the completion of tasks of daily life. However, it is still unclear how this quantity is regulated at the knee during dynamic tasks. In this work, we introduce a method to estimate the mechanical impedance of spring-mass systems using a torque-controllable exoskeleton with the intention of extending these methods to characterize the mechanical impedance of the human knee during locomotion. We characterize system bandwidth and intrinsic impedance, and present a perturbation-based methodology to identify the mechanical impedance of known spring-mass systems. Our approach was able to obtain accurate estimates of stiffness and inertia, with errors under 3% and ~13-16%, respectively. This work provides a qualitative and quantitative foundation that will enable accurate estimates of knee joint impedance during locomotion in future works.

Transfer of Impurities Determination Methods: Comparative Testing, Validation, Acceptance Criteria (Review)

Introduction. Different approaches are used for transfer of impurities determination methods. In most cases, comparative testing of samples or partial validation of methods is performed. At the same time, a number of issues important for practice are still relevant.Text. The features of methods validation and comparative testing of samples during the transfer of impurities determination methods are considered. Potential acceptance criteria – requirements to the permissible difference between results of transmitting and receiving laboratories – are given. The calculation formulas of the TOST test are considered, and the critical condition for the comparative testing of samples is given. The key points that should be taken into account when transferring the methods are discussed.Conclusion. The data and recommendations are presented, which are important for increasing the reliability of the transfer of the impurities determination methods.

Experience in Validation of Methods for Determination of Radiochemical Impurities in Radiopharmaceuticals

Most important quality attributes of any radiopharmaceutical (RPh) are its radiochemical purity (RCP) or content of radiochemical impurities (RCIs) that have to comply with respective norms and limits. However, at present, there is no unified approach to validation of analytical methods in the context of highly radioactive samples.The aim of the study was to develop an approach to validation of methods for determination of RCI content in RPhs.Materials and methods: the authors determined the content of RCIs in a radiopharmaceutical formulation containing a complex of technetium-99m and methylenediphosphonic acid by the radiometric method after isolation of impurities from the main compound by thin-layer chromatography using silica gel and methyl ethyl ketone (for sodium pertechnetate determination) and silica gel and 13.6% sodium acetate solution (for determination of hydrolysed reduced technetium-99m). The radioactivity was registered by a chromatogram scanner with a detector of gamma-rays with energies from 0.05 to 1.5 MeV.Results: the paper analyses existing official approaches to validation of analytical procedures and compares them with the results of experimental studies described in available publications. It assesses the validation parameters for compliance with the acceptance criteria set forth in the current regulations and substantiates selectivity of chromatographic determination of impurities under the selected test conditions. Coefficients of variation for repeatability, reproducibility, and accuracy did not exceed 4.5, 2.8, and 8.9%, respectively, given the relative error of not more than 10.5%. The study demonstrated signal linearity for the 10-fold dilution of the standardised sodium pertechnetate solution, it also demonstrated correspondence between the applied and detected radioactivity when performing the test in the impurity content range of 0.5–5%. The validation procedure was associated with significant radiation burden for the personnel of the quality control laboratory.Conclusions: the authors suggested a methodological approach to validation of methods for determination of RCI content in technetium-99m-based RPhs. This approach may be used in the development of a guideline on validation of analytical methods for RCP/RCI determination in RPhs, or for introduction of relevant sections into existing documents.